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Lithium Hydroxide → HCID 59577007, 화합물

HRID 2041978
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HRID 2041978 반응식
[C:1]([C:5]1[CH:22]=[CH:21][CH:20]=[CH:19][C:6]=1[O:7][CH:8]1[CH2:11][N:10]([C:12](=[O:18])[C:13]([O:15]CC)=[O:14])[CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Li+]>C(O)C>[C:1]([C:5]1[CH:22]=[CH:21][CH:20]=[CH:19][C:6]=1[O:7][CH:8]1[CH2:9][N:10]([C:12](=[O:18])[C:13]([OH:15])=[O:14])[CH2:11]1)([CH3:4])([CH3:2])[CH3:3]
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4

반응물 2

HCID 3939Lithium HydroxideHCID 59577194HCID 59577194, 화합물

생성물 1

HCID 59577007HCID 59577007, 화합물수율 65%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
0 °C

실험 절차

To a stirred solution of ethyl 2-(3-(2-tert-butylphenoxy)azetidin-1-yl)-2-oxoacetate (1.65 g, 5.40 mmol) in ethanol (60.0 ml) was added lithium hydroxide (16.2 mL of 1.0 M solution in water, 16.2 mmol) at room temperature. After 1 h the reaction mixture was concentrated under reduced pressure, the resulting residue was diluted with water, cooled to 0° C., adjusted to about pH 1 with 1.0 N hydrochloric acid and the resulting solution was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride, dried (Na2SO4), filtered and concentrated under reduced pressure. The residue was recrystallized from heptane/ethyl acetate to provide 2-(3-(2-tert-butylphenoxy)azetidin-1-yl)-2-oxoacetic acid (0.97 g, 65%) as a white powder.

후처리

  1. concentrationAfter 1 h the reaction mixture was concentrated under reduced pressure
  2. additionthe resulting residue was diluted with water
  3. extractionthe resulting solution was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated sodium chloride
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was recrystallized from heptane/ethyl acetate

출처 및 근거

ORD 기록
ord-a5ad544785d34beb93db8da0dae66deb
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586571B2

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